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Tetrahydrofuran → 2-(2-Tert-butoxycarbonylaminomethylthiophen-5-yl)carbonyl-4-chloroaniline

HRID 275854
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 275854
O1CCCC1.CN(OC)[C:8](=[O:17])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[NH2:16].Br[C:21]1[S:22][C:23]([CH2:26][NH:27][C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])=[CH:24][CH:25]=1.C([Li])CCC>C(OC(=O)C)C.O.CCCCCC>[C:31]([O:30][C:28]([NH:27][CH2:26][C:23]1[S:22][C:21]([C:8]([C:9]2[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=2[NH2:16])=[O:17])=[CH:25][CH:24]=1)=[O:29])([CH3:34])([CH3:32])[CH3:33]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 8028TetrahydrofuranHCID 2779810tert-Butyl ((5-bromothiophen-2-yl)methyl)carbamateHCID 222266052-amino-5-chloro-N-methoxy-N-methylbenzamideHCID 178418339Butyllithium

Produkt 1

HCID 183153332-(2-Tert-butoxycarbonylaminomethylthiophen-5-yl)carbonyl-4-chloroanilineAusbeute 7,3 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 8058HexaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A tetrahydrofuran (60 ml) solution of N-methyl-N-methyloxy-2-amino-5-chlorobenzamide (4.96 g) and 2-bromo-5-tert-butoxycarbonylaminomethylthiophene (5.45 g) was cooled to −78° C. To the solution was gradually added dropwise a hexane solution of n-butyl lithium (1.6 mol/L) (47 ml). To the mixture were further added water (200 ml) and acetic acid ethyl ester (200 ml). The organic layer was washed with water and dried over anhydrous MgSO4, followed by distilling off the solvent. The residual oily compound was purified by means of a silica gel column chromatography to give 2-(2-tert-butoxycarbonylaminomethylthiophen-5-yl)carbonyl-4-chloroaniline (0.5 g) as a yellow oily product. To a methanol (8 ml) solution of this product (0.15 g) was added sodium borohydride (60 mg). The mixture was stirred for 30 minutes at room temperature, to which was added acetic acid ethyl ester (100 ml). The mixture was washed with water and dried over anhydrous MgSO4. The solvent was then distilled off. To a methanol (5 ml) solution of the residue were added 4-biphenylcarbaldehyde (100 mg) and acetic acid (40 mg). The mixture was stirred for 10 minutes at room temperature, to which was added sodium cyano borohydride (40 mg). The mixture was stirred for 30 minutes at 60° C., to which was added acetic acid ethyl ester (50 ml). The mixture was washed with water and dried over anhydrous MgSO4. The solvent was then distilled off to leave 0.2 g of a residual compound.

Aufarbeitung

  1. washThe organic layer was washed with water
  2. dry with materialdried over anhydrous MgSO4
  3. distillationby distilling off the solvent
  4. customThe residual oily compound was purified by means of a silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-78487c25e3104edaabeb6a076bdcb343
Quelldatensatz
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06352982B1

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